CN103468154B - High-temperature-resistant room temperature curing phosphate adhesive and preparation method thereof - Google Patents
High-temperature-resistant room temperature curing phosphate adhesive and preparation method thereof Download PDFInfo
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- CN103468154B CN103468154B CN201310378767.3A CN201310378767A CN103468154B CN 103468154 B CN103468154 B CN 103468154B CN 201310378767 A CN201310378767 A CN 201310378767A CN 103468154 B CN103468154 B CN 103468154B
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Abstract
The invention discloses a high-temperature-resistant room temperature curing phosphate adhesive and a preparation method thereof, and relates to an adhesive and a preparation method thereof. The adhesive and the preparation method aim at solving the problems that the high-temperature-resistant adhesive prepared by the existing method cannot be cured easily at a room temperature, or the mechanical property and the heat resistance at a high temperature are poor after room temperature curing, and the preparation method is complicated. The high-temperature-resistant room temperature curing phosphate adhesive is prepared by modified aluminium dihydrogen phosphate and a curing agent. The preparation method comprises the steps that 1, aluminium hydroxide powder is added to a phosphoric acid solution; reaction is performed at 90-100 DEG C; chromic oxide is added; the reaction is continued at 90-100 DEG C; a modified aluminium dihydrogen phosphate solution is obtained; 2, aluminium nitride, yttrium oxide, calcium fluoride, boron nitride and zinc oxide are added to aluminium oxide, and mixed uniformly; the curing agent is obtained; and 3, the prepared modified aluminium dihydrogen phosphate solution and the curing agent are mixed uniformly, and stand at the room temperature; and the high-temperature-resistant room temperature curing phosphate adhesive is obtained. The adhesive is used for the fields of high-temperature-resistant ceramic material bonding and wood fire prevention coating.
Description
Technical field
The present invention relates to a kind of tackiness agent and preparation method thereof.
Background technology
Sizing agent is by the sticking and the interior poly-effect that waits of interface, and can make two or more product or natural or synthetic, the organic or inorganic class material that links together of material.At present high temperature resistant 1000 DEG C of above tackiness agent mainly contain Phosphoric Acid-Copper Oxide adhesive system, silicate adhesive system and phosphate adhesive system.Under Phosphoric Acid-Copper Oxide adhesive system room temperature, be difficult to solidify, conventionally need heating to solidify; Although silicate adhesive can self-vulcanizing, high temperature more than 1000 DEG C under condition mechanical property lower, shearing resistance is low, therefore, resistance toheat and water resistance are poor, and viscosity is large, be difficult for stirring and operation, cannot meet the requirement to mechanical property of adhering part.And existing preparation method's complex process, is not easy to operation.
Summary of the invention
The present invention is in order to solve difficult solidifying under high-temperature resistance adhesive room temperature prepared by existing method, or after self-vulcanizing in the time that high temperature is more than 1000 DEG C mechanical property and resistance toheat poor, cannot meet the requirement to mechanical property of adhering part, and the problem of preparation method's complexity, and high temperature resistant self-vulcanizing phosphate adhesive of the one providing and preparation method thereof.
One of the present invention is high temperature resistant self-vulcanizing phosphate adhesive, it is made up of modified phosphate aluminum dihydrogen and solidifying agent; Wherein, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150-200.
Described modified phosphate aluminum dihydrogen is made according to the following steps: one, take the phosphoric acid solution that mass fraction is 80-100 part, aluminium hydroxide pressed powder and the mass fraction that mass fraction is 20-50 part is the chromic oxide of 0.1-10 part; Two, the phosphoric acid solution taking is joined in reaction flask, then add aluminium hydroxide pressed powder, at 90-100 DEG C, react 1-1.5h, then add chromic oxide, at 90-100 DEG C, continue reaction 1.5-2h, prepare modified phosphate aluminum dihydrogen solution; Wherein, phosphoric acid solution massfraction is 70%-85%.
Described one is high temperature resistant self-vulcanizing phosphate adhesive, it is characterized in that making after described solidifying agent mixes aluminum oxide, aluminium nitride, yttrium oxide, Calcium Fluoride (Fluorspan), boron nitride and zinc oxide, each constituent mass umber is: 50-100 part aluminum oxide, 0.1-20 part aluminium nitride, 0.1-10 part yttrium oxide, 0.1-10 part Calcium Fluoride (Fluorspan), 0.1-5 part boron nitride and 0.1-5 part zinc oxide.
The preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive of the present invention carries out according to the following steps:
Step 1: prepare modified phosphate aluminum dihydrogen solution: take the phosphoric acid solution that mass fraction is 80-100 part, aluminium hydroxide pressed powder and the mass fraction that mass fraction is 20-50 part is the chromic oxide of 0.1-10 part; The phosphoric acid solution taking is joined in reaction flask, then add aluminium hydroxide pressed powder, at 90-100 DEG C, react 1-1.5h, then add chromic oxide, at 90-100 DEG C, continue reaction 1.5-2h, prepare modified phosphate aluminum dihydrogen solution; Wherein, phosphoric acid solution massfraction is 70%-85%;
Step 2: prepare solidifying agent: add aluminium nitride, yttrium oxide, Calcium Fluoride (Fluorspan), boron nitride and zinc oxide in aluminum oxide, mix, obtain solidifying agent; Wherein, each constituent mass umber is: 50-100 part aluminum oxide, 0.1-20 part aluminium nitride, 0.1-10 part yttrium oxide, 0.1-10 part Calcium Fluoride (Fluorspan), 0.1-5 part boron nitride and 0.1-5 part zinc oxide;
Step 3: modified phosphate aluminum dihydrogen solution and the solidifying agent of above-mentioned preparation are mixed, obtain high temperature resistant self-vulcanizing phosphate adhesive; Wherein, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150-200, and room temperature lower set time is 46-50h.
The present invention comprises following beneficial effect:
A kind of high temperature resistant self-vulcanizing phosphate adhesive of the present invention is be applied to high temperature ceramic material bonding, and a kind of sizing agent of fire retarding wood protection coating, this tackiness agent is taking modified phosphate aluminum dihydrogen as main body, taking aluminum oxide, aluminium nitride, yttrium oxide, Calcium Fluoride (Fluorspan), boron nitride and zinc oxide etc. as solidifying agent, solidification value is low, ambient temperature curable, and in the time that high temperature is more than 1000 DEG C, shearing resistance large (as shown in the table), mechanical property is high.In the air ambient that is warming up to 1300 DEG C with 10 DEG C/min, thermal weight loss is 7～10%, and maximum operation (service) temperature can reach 1500 DEG C, has good water resistance and resistance toheat.In addition, viscosity is low, is easy to stir and operation, can meet the requirement to mechanical property of adhering part, and thermal insulation tile material, titanium alloy and C/C matrix material are had to good adhesiveproperties.Preparation method's of the present invention technique is simple, easy handling.
Note: 1) " * " represents that material is destroyed, intensity when numerical value is material damage;
2) "---" represents not test;
3) test result of 1300 DEG C and 1500 DEG C is incubated after 20min at this temperature, room temperature test result, and all the other are on-line testing result.
Concrete implementation step:
Embodiment one: the high temperature resistant self-vulcanizing phosphate adhesive of one of present embodiment, is characterized in that it is made up of modified phosphate aluminum dihydrogen and solidifying agent; Wherein, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150-200.
Embodiment two: present embodiment is different from embodiment one: described modified phosphate aluminum dihydrogen and the mass ratio of solidifying agent are 100:150.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one or two: described modified phosphate aluminum dihydrogen is made according to the following steps: one, take the phosphoric acid solution that mass fraction is 80-100 part, aluminium hydroxide pressed powder and the mass fraction that mass fraction is 20-50 part is the chromic oxide of 0.1-10 part; Two, the phosphoric acid solution taking is joined in reaction flask, then add aluminium hydroxide pressed powder, at 90-100 DEG C, react 1-1.5h, then add chromic oxide, at 90-100 DEG C, continue reaction 1.5-2h, prepare modified phosphate aluminum dihydrogen solution; Wherein, phosphoric acid solution massfraction is 70%-85%.Other is identical with embodiment one or two.
Embodiment four: present embodiment is different from one of embodiment one to three: phosphoric acid solution mass fraction is 100 parts, aluminium hydroxide pressed powder mass fraction is 40 parts, chromic oxide mass fraction is 3 parts.Other is identical with one of embodiment one to three.
Embodiment five: present embodiment is different from one of embodiment one to four: add the reaction times after aluminium hydroxide pressed powder to be 1.5h.Other is identical with one of embodiment one to four.
Embodiment six: present embodiment is different from one of embodiment one to five: phosphoric acid solution quality percentage composition is 85%.Other is identical with one of embodiment one to five.
Embodiment seven: present embodiment is different from one of embodiment one to six: described solidifying agent is made after aluminum oxide, aluminium nitride, yttrium oxide, Calcium Fluoride (Fluorspan), boron nitride and zinc oxide are mixed, each constituent mass umber is: 50-100 part aluminum oxide, 0.1-20 part aluminium nitride, 0.1-10 part yttrium oxide, 0.1-10 part Calcium Fluoride (Fluorspan), 0.1-5 part boron nitride and 0.1-5 part zinc oxide.Other is identical with one of embodiment one to six.
Embodiment eight: present embodiment is different from one of embodiment one to seven: the each constituent mass umber of solidifying agent is respectively: aluminum oxide is 100 parts, aluminium nitride is that 10 parts, yttrium oxide are that 5 parts, Calcium Fluoride (Fluorspan) are that 2 parts, boron nitride are that 2 parts, zinc oxide are 0.5 part.Other is identical with one of embodiment one to seven.
Embodiment nine: the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive of present embodiment, is characterized in that it is to carry out according to the following steps:
Step 1: prepare modified phosphate aluminum dihydrogen solution: take the phosphoric acid solution that mass fraction is 80-100 part, aluminium hydroxide pressed powder and the mass fraction that mass fraction is 20-50 part is the chromic oxide of 0.1-10 part; The phosphoric acid solution taking is joined in reaction flask, then add aluminium hydroxide pressed powder, at 90-100 DEG C, react 1-1.5h, then add chromic oxide, at 90-100 DEG C, continue reaction 1.5-2h, prepare modified phosphate aluminum dihydrogen solution; Wherein, phosphoric acid solution massfraction is 70%-85%;
Step 2: prepare solidifying agent: add aluminium nitride, yttrium oxide, Calcium Fluoride (Fluorspan), boron nitride and zinc oxide in aluminum oxide, mix, obtain solidifying agent; Wherein, each constituent mass umber is: 50-100 part aluminum oxide, 0.1-20 part aluminium nitride, 0.1-10 part yttrium oxide, 0.1-10 part Calcium Fluoride (Fluorspan), 0.1-5 part boron nitride and 0.1-5 part zinc oxide;
Step 3: modified phosphate aluminum dihydrogen solution and the solidifying agent of above-mentioned preparation are mixed, obtain high temperature resistant self-vulcanizing phosphate adhesive; Wherein, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150-200, and room temperature lower set time is 46-50h.
Embodiment ten: present embodiment is different from embodiment nine: in step 1, phosphoric acid solution mass fraction is 100 parts, aluminium hydroxide pressed powder mass fraction is 40 parts, chromic oxide mass fraction is 3 parts.Other is identical with embodiment nine.
Embodiment 11: present embodiment is different from embodiment nine or ten: the reaction times in step 1 is 1.5h.Other is identical with embodiment nine or ten.
Embodiment 12: present embodiment is different from one of embodiment nine to 11: the phosphoric acid solution quality percentage composition described in step 1 is 85%.Other is identical with one of embodiment nine to 11.
Embodiment 13: present embodiment is different from one of embodiment nine to 12: in step 2, the each constituent mass umber of solidifying agent is respectively: aluminum oxide is 100 parts, aluminium nitride is that 10 parts, yttrium oxide are that 5 parts, Calcium Fluoride (Fluorspan) are that 2 parts, boron nitride are that 2 parts, zinc oxide are 0.5 part.Other is identical with one of embodiment nine to 12.
Embodiment 14: present embodiment is different from one of embodiment nine to 13: in described step 3, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150.Other is identical with one of embodiment nine to 13.
Embodiment 15: present embodiment is different from one of embodiment nine to 14: in described step 3, room temperature lower set time is 48h.Other is identical with one of embodiment nine to 14.
Embodiment 1
The preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive of the present embodiment, carries out according to the following steps:
Step 1: 100 part of 85% phosphoric acid solution joined in reaction flask, then slowly add 40 parts of aluminium hydroxide pressed powders, at 90-100 DEG C, react 1.5h, then add 3 parts of chromic oxide, at 90-100 DEG C, continue reaction 1.5h, prepare modified phosphate aluminum dihydrogen solution;
Step 2: add 10 parts of aluminium nitride, 5 parts of yttrium oxide, 2 parts of Calcium Fluoride (Fluorspan), 2 parts of boron nitride and 0.5 part of zinc oxide in 100 parts of aluminum oxide, obtain solidifying agent after mixing.
Step 3: modified phosphate aluminum dihydrogen solution and the solidifying agent of above-mentioned preparation are mixed, obtain high temperature resistant self-vulcanizing phosphate adhesive.Wherein, the modified phosphate aluminum dihydrogen solution adding and the mass ratio of solidifying agent are 100:150, and the self-vulcanizing time is 48h.
The high temperature resistant self-vulcanizing phosphate adhesive of gained is carried out to the test of resistance toheat and water resistance, and test result is as follows:
(1) resistance toheat: be warming up to 1300 DEG C with 10 DEG C/min under air ambient, thermal weight loss is 7～10%.
(2) water resistance: by being soaked in the tap water of room temperature 3 days by sticky material, then test shearing resistance, result is as shown in the table:
Note: 1) " * " represents that material is destroyed, intensity when numerical value is material damage;
2) "---" represents not test;
3) test result of 1300 DEG C and 1500 DEG C is incubated after 20min at this temperature, room temperature test result, and all the other are on-line testing result.
Result shows, the high temperature resistant self-vulcanizing phosphate adhesive of the present embodiment gained, and mechanical property is high, and resistance toheat and water resistance are strong, and solidification value is low, ambient temperature curable.And viscosity is low, be easy to stir and operation, can meet the requirement to mechanical property of adhering part.Preparation method's technique is simple, easy handling.Thermal insulation tile material, titanium alloy and C/C matrix material are had to good adhesiveproperties.
Claims (8)
1. prepare a method for high temperature resistant self-vulcanizing phosphate adhesive, it is characterized in that it is to carry out according to the following steps:
Step 1: prepare modified phosphate aluminum dihydrogen solution: take the phosphoric acid solution that mass fraction is 80-100 part, aluminium hydroxide pressed powder and the mass fraction that mass fraction is 20-50 part is the chromic oxide of 0.1-10 part; The phosphoric acid solution taking is joined in reaction flask, then add aluminium hydroxide pressed powder, at 90-100 DEG C, react 1-1.5h, then add chromic oxide, at 90-100 DEG C, continue reaction 1.5-2h, prepare modified phosphate aluminum dihydrogen solution; Wherein, phosphoric acid solution massfraction is 70%-85%;
Step 2: prepare solidifying agent: add aluminium nitride, yttrium oxide, Calcium Fluoride (Fluorspan), boron nitride and zinc oxide in aluminum oxide, mix, obtain solidifying agent; Wherein, each constituent mass umber is: 50-100 part aluminum oxide, 0.1-20 part aluminium nitride, 0.1-10 part yttrium oxide, 0.1-10 part Calcium Fluoride (Fluorspan), 0.1-5 part boron nitride and 0.1-5 part zinc oxide;
Step 3: modified phosphate aluminum dihydrogen solution and the solidifying agent of above-mentioned preparation are mixed, obtain high temperature resistant self-vulcanizing phosphate adhesive; Wherein, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150-200, and room temperature lower set time is 46-50h.
2. the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive according to claim 1, it is characterized in that in described step 1, phosphoric acid solution mass fraction is 100 parts, aluminium hydroxide pressed powder mass fraction is 40 parts, and chromic oxide mass fraction is 3 parts.
3. the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive according to claim 2, is characterized in that adding the reaction times after aluminium hydroxide pressed powder to be 1.5h in described step 1.
4. the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive according to claim 3, is characterized in that in described step 1, phosphoric acid solution quality percentage composition is 85%.
5. the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive according to claim 4, it is characterized in that the quality of alumina umber in described step 2 is 100 parts, aluminium nitride mass fraction is that 10 parts, yttrium oxide mass fraction are that 5 parts, Calcium Fluoride (Fluorspan) mass fraction are that 2 parts, boron nitride quality umber are that 2 parts, zinc oxide mass fraction are 0.5 part.
6. the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive according to claim 5, in the step 3 described in it is characterized in that, the mass ratio of modified phosphate aluminum dihydrogen and solidifying agent is 100:150.
7. the preparation method of a kind of high temperature resistant self-vulcanizing phosphate adhesive according to claim 6, is characterized in that in described step 3 that room temperature lower set time is 48h.
8. the prepared high temperature resistant self-vulcanizing phosphate adhesive of one of preparation method as arbitrary in claim 1-7.
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| CN101426872B (en) * | 2007-02-15 | 2011-08-31 | 中国科学院过程工程研究所 | High temperature resistant inorganic composite adhesive |
| CN101358111B (en) * | 2008-08-27 | 2011-09-21 | 黑龙江省科学院石油化学研究院 | Phosphates adhesive and preparation method thereof |
| CN102352190B (en) * | 2011-06-16 | 2013-06-05 | 北京航空航天大学 | Microwave solidification type bonding agent and microwave solidification method thereof |
| CN102391792B (en) * | 2011-09-29 | 2013-06-05 | 哈尔滨工业大学 | Organic silicon resin/ phosphate composite adhesive and preparation method thereof |
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Inventor after: Chen Zeming Inventor after: Wang Chao Inventor after: Cao Xianqi Inventor after: Li Bohong Inventor after: Wang Wenbo Inventor after: Wang Xu Inventor after: Li Bing Inventor before: Chen Zeming Inventor before: Wang Chao Inventor before: Cao Xianqi Inventor before: Li Bohong Inventor before: Wang Wenbo |
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